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Thionyl Chloride → 1-(2,2,2-Trifluoroethoxy)-2-naphthoyl Chloride

HRID 1973190
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인쇄 미리보기

반응식

HRID 1973190 반응식
[F:1][C:2]([F:19])([F:18])[CH2:3][O:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[C:15](O)=[O:16].S(Cl)([Cl:22])=O>CN(C)C=O>[F:1][C:2]([F:19])([F:18])[CH2:3][O:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[C:15]([Cl:22])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 214931531-(2,2,2-Trifluoroethoxy)-2-Naphthoic Acid

생성물 1

HCID 214931501-(2,2,2-Trifluoroethoxy)-2-naphthoyl Chloride

시약·촉매·용매 1

HCID 6228Dimethylformamide촉매

실험 절차

A mixture of 10 g. (37 mmoles) of 1-(2,2,2-trifluoroethoxy)-2-naphthoic acid, 21.8 ml. (35.7 g., 300 mmoles) of purified thionyl chloride and 3 drops of dimethylformamide is refluxed for one hour. Excess thionyl chloride is removed in vacuo at water aspirator pressure while heating on a steam bath. Last traces of thionyl chloride are removed by vacuum distillation with added benzene. The product is 1-(2,2,2-trifluoroethoxy)-2-naphthoyl chloride according to infrared spectral measurement.

후처리

  1. additionA mixture of 10 g
  2. customExcess thionyl chloride is removed in vacuo at water aspirator pressure
  3. temperaturewhile heating on a steam bath
  4. customLast traces of thionyl chloride are removed by vacuum distillation with added benzene

출처 및 근거

ORD 기록
ord-afc3b72f7eb447d487f21eface9e9990
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03996280

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